Method for determining solvents residual in acotiamide hydrochloride bulk drug

A technology for acotiamide hydrochloride and residual solvents, applied in the field of determination of residual solvents in acotiamide hydrochloride raw materials, can solve problems that need to be improved, achieve rapid and efficient separation and content determination, high accuracy, and good quality assurance Effect

Inactive Publication Date: 2018-03-30
WATERSTONE PHARMA WUHAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, the method for determining the residual solvent in acotiamide hydrochloride bulk drug still needs to be improved

Method used

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  • Method for determining solvents residual in acotiamide hydrochloride bulk drug
  • Method for determining solvents residual in acotiamide hydrochloride bulk drug
  • Method for determining solvents residual in acotiamide hydrochloride bulk drug

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Instrument: Agilent 7890A-7697A headspace gas chromatograph, FID detector;

[0050]Chromatographic column: DB-624 (30m*0.53mm, 3.0μm);

[0051] Chromatographic parameters: carrier gas: nitrogen; carrier gas flow rate: 2.0ml / min; split ratio: 10:1;

[0052] Detector temperature: 250°C; Injection port temperature: 200°C;

[0053] Column temperature: the initial temperature is 40°C and kept for 5 minutes, then raised to 220°C at a rate of 20°C / min, and kept for 5 minutes;

[0054] Headspace detection parameters: heating box temperature: 80°C; quantitative loop temperature: 100°C; transfer line temperature: 110°C;

[0055] Headspace equilibration time: 20min; Cycle time: 30min; Injection time: 1.0min;

[0056] Pressure balance time: 0.2min.

[0057] 1. Methodological specificity

[0058] Blank solution: dimethylsulfoxide (DMSO).

[0059] Methanol stock solution: take about 0.30g of methanol, weigh it accurately, put it in a 50ml measuring bottle, dilute and dissolve i...

Embodiment 2

[0094] Instrument: Agilent 7890A-7697A headspace gas chromatograph, FID detector;

[0095] Chromatographic column: DB-624 (30m*0.53mm, 3.0μm);

[0096] Chromatographic parameters: carrier gas: nitrogen; carrier gas flow rate: 2.0ml / min; split ratio: 1:1;

[0097] Detector temperature: 260°C; Injection port temperature: 200°C;

[0098] Column temperature: the initial temperature is 35°C and kept for 5 minutes, then raised to 220°C at a rate of 20°C / min, and kept for 5 minutes.

[0099] Headspace detection parameters: heating box temperature: 80°C; quantitative loop temperature: 100°C; transfer line temperature: 110°C;

[0100] Headspace equilibration time: 20min; Cycle time: 30min; Injection time: 1.0min;

[0101] Pressure balance time: 0.1min.

[0102] experiment procedure:

[0103] Blank solution: dimethylsulfoxide (DMSO).

[0104] System suitability solution: Precisely pipette 1.0ml of each stock solution in Example 1 into a 50ml volumetric flask filled with about 30ml...

Embodiment 3

[0109] Instrument: Agilent 7890A-7697A headspace gas chromatograph, FID detector;

[0110] Chromatographic column: DB-624 (30m*0.53mm, 3.0μm);

[0111] Chromatographic parameters: carrier gas: nitrogen; carrier gas flow rate: 2.0ml / min; split ratio: 1:1;

[0112] Detector temperature: 260°C; Injection port temperature: 200°C;

[0113] Column temperature: the initial temperature is 45°C and kept for 5 minutes, then raised to 220°C at a rate of 20°C / min, and kept for 5 minutes.

[0114] Headspace detection parameters: heating box temperature: 80°C; quantitative loop temperature: 100°C; transfer line temperature: 110°C;

[0115] Headspace equilibration time: 20min; Cycle time: 30min; Injection time: 1.0min;

[0116] Pressure balance time: 0.1min.

[0117] experiment procedure:

[0118] Blank solution: dimethylsulfoxide (DMSO).

[0119] System suitability solution: Precisely pipette 1.0ml of each positioning solution in Example 1 into a 50ml volumetric flask filled with about ...

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Abstract

The invention discloses a method for determining solvents residual in an acotiamide hydrochloride bulk drug. The method adopts the following analysis conditions: the chromatographic column adopts a capillary chromatographic column with 6% cyanopropylphenyl 94% polydimethylsiloxane as the stationary phase; a reference substance solution is injected multiple times in a split flow manner, a sample solution is injected in the split flow manner, the carrier gas is nitrogen, the introduction is carried out by using a headspace injector, and detection is performed after temperature programming; and the detector adopts an FID detector. Methanol, isopropanol, dichloromethane and toluene in the acotiamide hydrochloride bulk drug are rapidly and efficiently separated under same chromatographic conditions through the method in order to effectively control the quality of acotiamide hydrochloride. The detection method has the advantages of strong specificity, high detection sensitivity, high precision, high accuracy, convenience in operation, and effective control of the product quality.

Description

technical field [0001] The invention belongs to the technical field of drug analysis, in particular, the invention relates to a method for determining residual solvents in acotiamide hydrochloride crude drug. Background technique [0002] The chemical name of acotiamide is N-[2-(diisopropylamino)ethyl]-2-[(2-hydroxy-4,5-dimethoxybenzoyl)amino]-1,3 - the hydrochloride trihydrate of thiazole-4-carboxamide, its structural formula is: [0003] [0004] The organic solvents used in the production process of pharmaceutical raw materials and preparations but not completely removed in the end are collectively referred to as residual solvents. If the residual amount exceeds the safe value, it will have a certain impact on the human body of the patient. According to the degree of hazard, the ICH guidelines stipulate 4 types of solvents and their limit values. According to the residual solvent content requirements stipulated in the fourth part of the Chinese Pharmacopoeia 2015 edi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/74G01N30/86G01N30/06
CPCG01N30/06G01N30/74G01N30/8634
Inventor 高宏平杭健钱丽娜
Owner WATERSTONE PHARMA WUHAN
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